KR102387660B1 - A method for synthesizing hydroxyapatite using sludge that produced during the Li compound manufacturing process and the synthesizing hydroxyapatite thereof - Google Patents
A method for synthesizing hydroxyapatite using sludge that produced during the Li compound manufacturing process and the synthesizing hydroxyapatite thereof Download PDFInfo
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Abstract
Description
본 발명은 리튬화합물 제조 공정시 발생하여 폐기되는 인산칼슘 슬러지를 그 출발 원료로 하여 간단한 공정을 통해 고순도 수산화아파타이트 분말 제조 방법 및 이로부터 제조된 수산화아파타이트 분말에 관한 것이다.The present invention relates to a method for preparing high-purity hydroxyapatite powder through a simple process using calcium phosphate sludge generated and discarded during the lithium compound manufacturing process as a starting material, and to hydroxyapatite powder prepared therefrom.
무기질 수산화아파타이트는 인체의 뼈나 치아 등 경조직의 주요 무기 성분으로서 정형외과 및 치과 등의 의료분야에서 골 대체재로 널리 사용되고 있다. 그리고 의족, 의치 등의 코팅제로 이용되고 있다.Inorganic hydroxyapatite is a major inorganic component of hard tissues such as bones and teeth of the human body and is widely used as a bone substitute in medical fields such as orthopedics and dentistry. It is also used as a coating agent for prosthetic legs and dentures.
특히 수산화아파타이트는 입자가 미세하고 균일하여 석유화학제품(EPS, SAN 등)에 분산제로 첨가하여 사용되고 있다. 이외에 각종 흡습성 분말제품과 소금 등의 응결방지제, 식품이나 음료에 칼슘강화제, 그 외 사료첨가제 등에 사용되고 있다.In particular, hydroxyapatite has fine and uniform particles and is used as a dispersant in petrochemical products (EPS, SAN, etc.). In addition, it is used in various hygroscopic powder products, anti-caking agents such as salt, calcium fortifying agents in food and beverages, and other feed additives.
또한 단백질 핵산을 분리하기 위한 HPLC 컬럼의 충진제로 쓰이며 촉매나 가스 센서로 일부 사용한다고 보고된 바 있다. In addition, it has been reported that it is used as a filler for HPLC columns for separating protein and nucleic acids and partially used as a catalyst or gas sensor.
본 발명에서는 이와 같이 여러 방면에서 유용하게 사용되는 수산화아파타이트를 제공함에 있어, 리튬화합물 제조공정시 발생되어 폐기되는 인산칼슘 슬러지를 이용하여 보다 저렴한 비용으로 고순도의 수산화아파타이트를 제조할 수 있는 방법을 제공하고자 한다.In the present invention, in providing hydroxide apatite useful in various fields as described above, a method capable of producing high-purity hydroxide apatite at a lower cost using calcium phosphate sludge generated and discarded during the lithium compound manufacturing process is provided. want to
본 발명자는 이와 같이 리튬화합물 제조공정에서 발생하는 인산칼슘 슬러지와 인산(H3PO4)을 출발원료로 사용하여 이들을 직접 반응시켜서 수산화아파타이트를 제조하고자 하였다.The present inventor tried to prepare hydroxyapatite by directly reacting calcium phosphate sludge and phosphoric acid (H 3 PO 4 ) generated in the lithium compound manufacturing process as starting materials as described above.
이를 통해, 다량 배출되고 있는 슬러지로 인해 야기되는 환경 문제를 해결함과 아울러, 의료용 생체 재료로서 유용한 수산화아파타이트 분말을 저렴한 비용으로 제공하고자 한다.Through this, it is intended to solve the environmental problem caused by the large amount of sludge being discharged, and to provide hydroxyapatite powder useful as a medical biomaterial at a low cost.
본 발명은 전지용 원료인 리튬화합물 제조 공정시 발생하여 폐기되는 인산칼슘 슬러지를 그 출발 원료로 하여 간단한 공정을 통해 수산화아파타이트 분말을 제조하는 방법과 이에 따라 제조된 수산화아파타이트 분말을 제공하고자 하는 것을 발명의 목적으로 한다.An object of the present invention is to provide a method for preparing hydroxyapatite powder through a simple process using, as a starting material, calcium phosphate sludge, which is generated and discarded during the lithium compound manufacturing process, which is a raw material for batteries, and to provide the hydroxyapatite powder prepared accordingly. The purpose.
상기 목적을 달성하기 위하여,In order to achieve the above object,
본 발명은 리튬화합물 제조 공정시 발생하는 슬러지에 물(H2O)을 투입한 슬러지액을 부유선별하여 상기 슬러지액으로부터 SiO2, Al2O3, Fe2O3를 제거하는 단계(S10)와,The present invention is a step of removing SiO 2 , Al 2 O 3 , Fe 2 O 3 from the sludge solution by flotation of water (H 2 O) added to the sludge generated during the lithium compound manufacturing process (S10) Wow,
상기 단계(S10)를 거친 슬러지액에 인산(H3PO4)을 주입하여 상기 슬러지액에 포함되어 있는 물(H2O)을 용매로 습식반응시키되, 반응속도의 증진을 위해 기계화학적 활성화 분쇄과정을 거치는 단계(S20)와,Phosphoric acid (H 3 PO 4 ) is injected into the sludge liquid that has undergone the step (S10), and water (H 2 O) contained in the sludge liquid is wet-reacted with a solvent, but mechanically and chemically activated pulverization to increase the reaction rate A step of going through the process (S20) and,
상기 기계화학적 활성화 분쇄과정을 거친 후 여과하는 단계(S30)와,A step of filtering after the mechanochemical activation grinding process (S30) and;
상기 여과과정을 거친 후 건조하는 단계(S40)와,A step of drying after the filtration process (S40) and;
상기 건조과정을 거친 후 분쇄하는 단계(S50)를 포함하는, 리튬화합물 제조시의 슬러지를 이용한 고순도 수산화아파타이트 분말 제조 방법을 제공한다.Provided is a method for producing high-purity hydroxyapatite powder using sludge during lithium compound production, comprising the step of pulverizing after the drying process (S50).
또한, 상기 제조방법을 통해, 리튬화합물 제조시의 슬러지를 이용한 고순도 수산화아파타이트 분말을 제공한다.In addition, through the above production method, a high-purity hydroxide apatite powder using sludge during the production of a lithium compound is provided.
본 발명에 따른 리튬화합물 제조시의 인산칼슘 슬러지를 이용한 고순도 수산화아파타이트 분말 제조 방법 및 이에 따른 수산화아파타이트 분말은 기존의 복잡한 공정들을 거쳐 수산화아파타이트를 제조하는 종래의 방법과는 달리, 리튬화합물 제조시 발생하는 인산칼슘 슬러지에 직접 인산을 투여하여 증류수를 용매로 습식 반응시키고 반응속도 증진을 위해 기계화학적 활성화, 여과, 건조, 분쇄, 열처리를 통해 99% 이상의 고순도 수산화아파타이트를 훨씬 간단하게 제조할 수 있다는 장점을 갖는다.The method for producing high-purity hydroxide apatite powder using calcium phosphate sludge in the production of lithium compounds according to the present invention, and thus the hydroxide apatite powder according to the present invention, is generated during lithium compound production Phosphoric acid is directly administered to calcium phosphate sludge that is used in the process, and distilled water is wet-reacted as a solvent, and mechanical and chemical activation, filtration, drying, pulverization, and heat treatment are performed to increase the reaction rate. has
도 1은 본 발명에 따른 리튬화합물 제조시 발생하는 슬러지를 이용한 고순도 수산화아파타이트 분말 제조 공정도.1 is a process diagram for manufacturing high-purity hydroxyapatite powder using sludge generated during the production of a lithium compound according to the present invention.
이하, 본 발명에 따른 리튬화합물 제조시 발생하는 인산칼슘 슬러지를 이용한 고순도 수산화아파타이트 분말 제조 방법 및 이에 따른 수산화아파타이트 분말에 대해 구체적으로 살펴보도록 한다.Hereinafter, a method for producing high-purity hydroxyapatite powder using calcium phosphate sludge generated during the production of a lithium compound according to the present invention and the resulting hydroxyapatite powder will be described in detail.
상기한 바와 같이,As mentioned above,
본 발명에 따른 고순도 수산화아파타이트 분말 제조 방법은The method for producing high-purity hydroxyapatite powder according to the present invention
리튬화합물 제조 공정시 발생하는 인산칼슘 슬러지에 물(H2O)을 투입하여 부유선별을 통해 상기 슬러지로부터 SiO2, Al2O3, Fe2O3를 제거하는 단계(S10)와,Removing SiO 2 , Al 2 O 3 , Fe 2 O 3 from the sludge through flotation by adding water (H 2 O) to the calcium phosphate sludge generated during the lithium compound manufacturing process (S10);
상기 단계(S10)를 거친 슬러지액에 인산(H3PO4)을 주입하여 상기 물(H2O)을 용매로 습식반응시키되, 반응속도의 증진을 위해 기계화학적 활성화 분쇄과정을 거치는 단계(S20)와,Phosphoric acid (H 3 PO 4 ) is injected into the sludge liquid that has undergone the step (S10), and the water (H 2 O) is wet-reacted with a solvent, but subjected to a mechanochemical activation grinding process to increase the reaction rate (S20) )Wow,
상기 기계화학적 활성화 분쇄과정을 거친 후 여과하는 단계(S30)와,A step of filtering after the mechanochemical activation grinding process (S30) and;
상기 여과과정을 거친 후 건조하는 단계(S40)와,A step of drying after the filtration process (S40) and;
상기 건조과정을 거친 후 분쇄하는 단계(S50)를 포함한다.and pulverizing after the drying process (S50).
이하, 상기 고순도 수산화아파타이트 분말 제조 방법에 대해 각 단계별로 구체적으로 살펴보도록 한다.Hereinafter, each step of the manufacturing method of the high-purity hydroxyapatite powder will be described in detail.
[ 리튬화합물 제조 공정시 발생하는 인산칼슘 슬러지에 물(H[ Water (H) in calcium phosphate sludge generated during the lithium compound manufacturing process 22 O)을 투입한 슬러지액을 부유선별하는 단계(S10) ]Step of flotation of the sludge liquid into which O) was added (S10) ]
본 발명에 따른 고순도 수산화아파타이트 분말 제조 공정은 전지용 원료인 리튬화합물 제조 공정시 발생하여 폐기되는 인산칼슘 슬러지를 출발 물질로 한다. The high-purity hydroxide apatite powder manufacturing process according to the present invention uses, as a starting material, calcium phosphate sludge, which is generated and discarded during the manufacturing process of a lithium compound, which is a raw material for batteries.
상기 인산칼슘 슬러지를 이용한 고순도 수산화아파타이트 분말 제조를 위한 첫단계로서, S10단계에서는 상기 인산칼슘 슬러지에 물(H2O)을 투입한 슬러지액으로부터 SiO2, Al2O3, Fe2O3를 제거하는 단계이다.As a first step for producing high-purity hydroxyapatite powder using the calcium phosphate sludge, in step S10, SiO 2 , Al 2 O 3 , Fe 2 O 3 was prepared from the sludge solution in which water (H 2 O) was added to the calcium phosphate sludge. This is the removal step.
상기 S10단계의 부유선별은 부유선광기를 이용하여 유가광물의 철저한 분리, 불순물의 제거는 물론 높은 회수율로 원하는 성분을 얻기 위한 것이다.The flotation in step S10 is to obtain the desired component with a high recovery rate as well as thorough separation of valuable minerals and removal of impurities using a flotation machine.
일반적으로 부유선별은 광석으로부터 목적으로 하는 광물을 선택적으로 채집하는 방법의 하나이다. 고-액 또는 고-액-기 계면의 계면화학적 성질을 이용한 특정광물을 기포(bubble)에 부착시켜 부상분리하는 방법이다. In general, flotation is one of the methods of selectively collecting target minerals from ores. It is a method for flotation separation by attaching specific minerals to bubbles using the interfacial chemical properties of solid-liquid or solid-liquid-group interfaces.
광석은 각각의 입자가 단일의 광물이 되도록 수중에서 미세하게 분쇄시켜 광액(pulp) 상태로 만들며, 상기 광액에 포수제와 기포제를 적당량 첨가하여 격렬하게 교반시키면 상기 포수제에 의해 표면이 소수성화된 특정광물만 부착시켜 부상 및 회수한다.The ore is finely pulverized in water so that each particle becomes a single mineral to make a mineral liquid (pulp). Only specific minerals are attached to float and recover.
본 발명에 따른 부유선별은 슬러지에 물을 투입하되, 슬러지와 물의 비율이 1: 55 ~ 70 중량비를 이루도록 투입한다. In the flotation according to the present invention, water is added to the sludge, and the ratio of the sludge to water is 1: 55 to 70 by weight.
다음으로, 물이 투입된 슬러지액을 초음파 분쇄기(ultrasonic processor)를 이용하여 1 ~ 3 시간동안 초음파 분쇄과정을 거친다.Next, the sludge liquid into which water is added is subjected to an ultrasonic pulverization process for 1 to 3 hours using an ultrasonic processor.
다음으로, 초음파 분쇄과정을 거친 슬러지액 중 상층에서 부유하고 있는 부유물을 펌프를 이용하여 자력선별기로 이송한 후, 자력선별기를 통해 상기 슬러지액에 포함되어 있는 SiO2, Al2O3 및 Fe2O3를 선별하여 제거한다.Next, the suspended matter suspended in the upper layer of the sludge liquid that has undergone the ultrasonic grinding process is transferred to the magnetic separator by using a pump, and then SiO 2 , Al 2 O 3 and Fe 2 contained in the sludge liquid through the magnetic separator. O 3 is selected and removed.
[ 부유선별을 거친 후 인산(H[ After flotation, phosphoric acid (H 33 POPO 44 )을 주입하여 활성화 분쇄과정을 거치는 단계(S20) ]) to pass through an activated grinding process (S20) ]
본 단계(S10)를 거쳐 SiO2, Al2O3 및 Fe2O3가 제거된 슬러지액에 인산(H3PO4)을 주입하여 상기 슬러지액에 포함되어 있는 물(H2O)을 용매로 습식반응시키되,Phosphoric acid (H 3 PO 4 ) was injected into the sludge from which SiO 2 , Al 2 O 3 and Fe 2 O 3 were removed through this step (S10), and water (H 2 O) contained in the sludge was dissolved as a solvent. Wet reaction with
상기 습식반응의 반응속도 증진을 위해 기계화학적 활성화 분쇄과정을 거치는 단계이다.It is a step of undergoing a mechanochemical activation and pulverization process to increase the reaction rate of the wet reaction.
이때 상기 인산(H3PO4)의 주입량으로 슬러지액의 pH를 7~9.5로 조절하여 습식반응에 의한 침전이 일어날 수 있도록 한다.At this time, the pH of the sludge liquid is adjusted to 7 to 9.5 with the amount of phosphoric acid (H 3 PO 4 ) injected so that precipitation by the wet reaction can occur.
그리고 기계화학적 활성화 분쇄를 통해 분쇄 직후의 활성화된 표면에 의한 보다 강한 화학결합이 일어나도록 하기 위하여, 상기 인산을 주입한 후에는 기계화학적 활성화 분쇄과정을 거치게 된다.And in order to cause stronger chemical bonding by the activated surface immediately after pulverization through mechanochemically activated pulverization, the phosphoric acid is injected and then subjected to a mechanochemically activated pulverizing process.
상기 기계화학적 활성화 분쇄는 지속적인 볼밀링 공정으로 반응 입자의 크기를 작게하여 접촉면적을 증가시킴으로써 반응속도를 증진시키게 된다.The mechanochemical activation pulverization is a continuous ball milling process to increase the contact area by reducing the size of the reaction particles to increase the reaction rate.
이와 같은 메카노케미컬반응은 분쇄시에 가해졌던 대량의 에너지 일부가 고체 내에 축적되어, 결정의 구조부정이나 부정형화 등의 물질 변화를 일으키고, 그 활성화에 의해 반응성이 높아진다.In such a mechanochemical reaction, a large amount of energy applied during pulverization is accumulated in the solid, causing material changes such as structural irregularity or amorphization of crystals, and the reactivity is increased by activation.
상기 기계화학적 활성화 분쇄는 The mechanochemically activated grinding is
원심진동밀 또는 어트리션밀을 이용하여 메카노케미칼 분쇄처리를 하는 것으로서,As a mechanochemical grinding treatment using a centrifugal vibration mill or an attrition mill,
이 중 선택된 밀(Mill)에 슬러지액과, 상기 슬러지액의 pH 7~9.5, 전기전도도 350 ㎲/cm 이하의 조건이 되도록 인산(H3PO4)을 주입한 후,Phosphoric acid (H 3 PO 4 ) is injected so that the sludge solution and the sludge solution have a pH of 7 to 9.5 and electrical conductivity of 350 μs/cm or less to the selected mill among them,
상기 진동밀 내부에 충진된 볼(ball)을 이용하여 2~3시간 동안 교반 및 분쇄하여 0.1~0.3 mm의 활성화물을 생성하여 1~6시간 숙성시켜 기계화학적반응에 의한 수산화아파타이트를 제조한다.Using a ball filled in the vibrating mill, stirring and pulverizing for 2 to 3 hours to produce an activated substance of 0.1 to 0.3 mm is aged for 1 to 6 hours to prepare hydroxyapatite by a mechanochemical reaction.
상기 활성화물의 입도범위가 0.1 mm 미만인 경우에는 상기 입도범위를 충족시키기 위한 시간이 많이 소요되어 비경제적이고, 0.3 mm를 초과하게 되는 경우에는 반응속도의 증진을 기대하기 어려우므로, 상기 활성화물의 입도범위는 0.1~0.3 mm로 한정하는 것이 바람직하다.When the particle size range of the active material is less than 0.1 mm, it takes a lot of time to satisfy the particle size range, which is uneconomical, and when it exceeds 0.3 mm, it is difficult to expect improvement of the reaction rate, so It is preferable to limit it to 0.1-0.3 mm.
분쇄와 미분쇄에 소요되는 비용 중에 동력비의 비중이 크기 때문에 상기 입도범위를 조정하는 것은 매우 중요하다.It is very important to adjust the particle size range because the proportion of power cost among the costs required for pulverization and fine pulverization is large.
[ 활성화 분쇄과정을 거친 후 여과하는 단계(S30) ][Step of filtering after the activation grinding process (S30)]
본 단계(S30)는 상기 단계(S20)를 통해 수득한 활성화물을 여과처리하여 순수한 수산화아파타이트 분말을 수득하는 단계이다.This step (S30) is a step of obtaining pure hydroxide apatite powder by filtering the activated material obtained through the step (S20).
상기 여과처리는 필터프레스를 이용한다.The filtration treatment uses a filter press.
상기 필터프레스는 밀폐된 여과실내로 슬러지를 펌프로 압입하여, 여과판에 장착되어진 여과포를 통해 고체와 액체를 분리시키는 여과장치이다. 구조가 간단하고, 하나의 장치로 여러가지 원료를 여과할 수 있다는 장점이 있는 여과장치이다.The filter press is a filtration device that presses sludge into a closed filtration chamber with a pump, and separates solids and liquids through a filter cloth mounted on a filter plate. It is a filtration device that has a simple structure and has the advantage of being able to filter various raw materials with one device.
[ 여과과정을 거친 후 건조하는 단계(S40) ][Step of drying after filtration (S40)]
상기 여과과정을 거쳐 수득한 순수한 수산화아파타이트 분말은 건조과정을 거치게 된다.The pure hydroxyapatite powder obtained through the filtration process is dried.
S40단계의 건조는 80 ~ 100 ℃에서 10 ~ 25분 동안 이루어진다.The drying in step S40 is carried out at 80 ~ 100 ℃ for 10 ~ 25 minutes.
상기 건조온도가 80 ℃ 미만인 경우에는 건조 속도가 늦다는 문제가 있고, 100 ℃를 초과하게 되는 경우에는 비등(boiling)하는 문제가 있으므로, 상기 건조는 80 ~ 100 ℃에서 10 ~ 25분 동안 이루어지는 것이 바람직하다.When the drying temperature is less than 80 ℃, there is a problem that the drying rate is slow, and when it exceeds 100 ℃, there is a problem of boiling, so that the drying is performed at 80 to 100 ℃ for 10 to 25 minutes desirable.
[ 건조과정을 거친 후 분쇄하는 단계(S50) ][Step of grinding after drying (S50)]
상기 건조과정을 거친 후에는 상기 순수한 수산화아파타이트 분말을 기계적 분쇄법을 이용하여 재분쇄하게 된다.After the drying process, the pure hydroxyapatite powder is re-grinded using a mechanical grinding method.
이와 같은 재분쇄를 통해 상기 순수한 수산화아파타이트 분말은 5 ~ 40 ㎛ 미립상을 유지하게 된다.Through such re-pulverization, the pure hydroxyapatite powder is maintained in a 5-40 μm particulate form.
본 발명에 따른 리튬화합물 제조시의 슬러지를 이용한 고순도 수산화아파타이트 분말 제조 방법 및 이에 따른 수산화아파타이트 분말은 종래의 방법과는 달리, 리튬화합물 제조시 발생하는 인산칼슘 슬러지에 직접 인산을 투여하여 증류수를 용매로 습식 반응시키고 반응속도 증진을 위해 기계화학적 활성화, 여과, 건조, 분쇄, 열처리를 통해 고순도의 수산화아파타이트를 훨씬 간단하게 제조할 수 있다는 장점을 가짐으로써 산업상 이용가능성이 크다.The method for producing high-purity hydroxyapatite powder using sludge in the production of lithium compounds according to the present invention and the hydroxyapatite powder according to the present invention are different from the conventional methods by directly administering phosphoric acid to calcium phosphate sludge generated during the production of lithium compounds, and dissolving distilled water as a solvent. Industrial applicability is great as it has the advantage that high-purity hydroxyapatite can be prepared much more simply through mechanochemical activation, filtration, drying, pulverization, and heat treatment to increase the reaction rate.
Claims (7)
상기 단계(S10)를 거친 슬러지액에 인산(H3PO4)을 주입하여 상기 슬러지액에 포함되어 있는 물(H2O)을 용매로 습식반응시키되, 반응속도의 증진을 위해 기계화학적 활성화 분쇄과정을 거치는 단계(S20)와,
상기 기계화학적 활성화 분쇄과정을 거친 후 여과하는 단계(S30)와,
상기 여과과정을 거친 후 건조하는 단계(S40)와,
상기 건조과정을 거친 후 분쇄하는 단계(S50)를 포함하는 것을 특징으로 하는 리튬화합물 제조시의 슬러지를 이용한 고순도 수산화아파타이트 분말 제조 방법.
SiO 2 , Al 2 O 3 , and Fe 2 O 3 are removed from the sludge by flotation by flotation of the sludge liquid in which water (H 2 O) is added to the sludge generated during the lithium compound manufacturing process, but the ratio of sludge to water is 1 : After adding water to the sludge to achieve a weight ratio of 55 to 70, SiO 2 contained in the sludge solution subjected to ultrasonic grinding for 1 to 3 hours using an ultrasonic processor with water, Removing Al 2 O 3 and Fe 2 O 3 through wet magnetic separation (S10);
Phosphoric acid (H 3 PO 4 ) is injected into the sludge liquid that has undergone the step (S10), and water (H 2 O) contained in the sludge liquid is wet-reacted with a solvent, but mechanically and chemically activated pulverization to increase the reaction rate A step of going through the process (S20) and,
A step of filtering after the mechanochemical activation grinding process (S30) and;
A step of drying after the filtration process (S40) and,
A method for producing a high-purity hydroxyapatite powder using sludge in the production of a lithium compound, characterized in that it includes a step (S50) of pulverizing after the drying process.
S20단계의 인산(H3PO4)은 슬러지액의 pH가 7~9.5가 되도록 주입하는 것을 특징으로 하는 리튬화합물 제조시의 슬러지를 이용한 고순도 수산화아파타이트 분말 제조 방법.
The method according to claim 1,
Phosphoric acid (H 3 PO 4 ) in step S20 is injected so that the pH of the sludge solution becomes 7 to 9.5.
S20단계의 기계화학적 활성화 분쇄는
원심진동밀을 이용하여 메카노케미칼 분쇄처리를 하는 것으로서,
상기 원심진동밀에 슬러지액과, 상기 슬러지액의 pH 7~9.5, 전기전도도 350 ㎲/cm 이하의 조건이 되도록 인산(H3PO4)을 주입한 후,
상기 원심진동밀 내부에 충진된 볼(ball)을 이용하여 2~3시간 동안 교반 및 분쇄하여 0.1~0.3 mm의 활성화물을 생성하여 1~6시간 숙성시키는 것을 특징으로 하는 리튬화합물 제조시의 슬러지를 이용한 고순도 수산화아파타이트 분말 제조 방법.
The method according to claim 1,
Mechanochemically activated pulverization in step S20 is
As a mechanochemical grinding process using a centrifugal vibration mill,
Phosphoric acid (H 3 PO 4 ) is injected into the centrifugal vibrating mill so that the sludge solution and the sludge solution have a pH of 7 to 9.5 and an electrical conductivity of 350 μs/cm or less,
Sludge in the production of lithium compounds, characterized in that by using a ball filled in the centrifugal vibrating mill, stirring and pulverization for 2 to 3 hours to produce an activated substance of 0.1 to 0.3 mm and aging it for 1 to 6 hours A method for producing high-purity hydroxyapatite powder using
S40단계의 건조는 80~100 ℃에서 10~25분 동안 이루어지는 것을 특징으로 하는 리튬화합물 제조시의 슬러지를 이용한 고순도 수산화아파타이트 분말 제조 방법.
The method according to claim 1,
A method for producing high-purity hydroxyapatite powder using sludge in manufacturing a lithium compound, characterized in that the drying in step S40 is performed at 80 to 100° C. for 10 to 25 minutes.
S50단계의 분쇄는 기계적 분쇄법에 의해 5~40 ㎛ 미립상으로 분쇄하는 것을 특징으로 하는 리튬화합물 제조시의 슬러지를 이용한 고순도 수산화아파타이트 분말 제조 방법.
The method according to claim 1,
A method for producing high-purity hydroxyapatite powder using sludge in the production of lithium compounds, characterized in that the pulverization in step S50 is pulverized into 5-40 μm fine particles by a mechanical pulverization method.
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